Ascertain the solubility of the Ugi adduct in methanol, ethanol, acetonitrile, and tetrahydrofuran.
Procedure
Pipette ≈ 2mL of each solvent into four separate vials.
Gradually add Ugi adduct, using sterilized (alcohol rinsed) spatula, to each vial until solution no longer remains clear once shaken.
Once excess Ugi adduct sample settles towards the bottom of the vial, filter 1mL of clear saturated liquid for speed vac assay.
Material
Solvents: THF - Tetrahydrofuran, stabilized anhydrous 99.9%
Lot# B0307053 AcroOrganics Methanol Ethanol - 200 Proof
Catalog# 111 AG S200 111 USP 200 111000200 Pharmco-AAper Acetonitrile - HPLC - 99.9%
Lot# 75-05-8 AcroOrganics Hexane
Lot# 061507A BDH Choloform ≈ 99%
Batch# 00751LD Sigma Aldrich Acetone
Water (distilled) Solute:
Ugi Product first obtained in Exp099
Results
Solvent
Volume of the Solution (mL)
Weight of the empty vial (g)
Weight of the vial after solvent evaporation
Solubility of the Ugi product
Acetonitrile
1
2.21003
THF
0.5
2.2148
Ethanol
0.5
2.2112
Chloroform
1
2.20921
Methanol
1
2.21177
Hexane
1
2.21784
Water (distilled)
1
2.22357
Discussion
Cloudy solutions indicate points surpassing level of saturation.
Conclusion
Log
2008-08-18
11:39 - Ugi product recrystalized ad rid of any impurities.
11:54 - Materials gathered (Methanol, Ethanol, THF, Acetonitrile)
12:30 - 2mL of methanol measured into vile and ugi product added and mixed. AS
12:32 - 2mL of acetonitrile measured into vile and ugi product added and mixed. CT
12:37 - 2mL of THF measured into vile and ugi product added and mixed. Methanol cleared up. AS
12:39 - 2mL of ethanol measured into vile and ugi product added and mixed. CT
12:41 - More ugi added to methanol. As
12:43 - More ugi added to THF. AS
12:52 - More ugi added to THF. AS. All solutions appear saturated and cloudy.
6:00 - Solutions appear saturated with residue at the bottom of the viles. Each vile vortexed to insure complete mixing.
6:40 - Gather more materials to create more saturated solutions (Deionized water, Hexane, Chloroform, Acetone)
6:44 - 2mL of Chloroform measured into vile and ugi product added and vortexed. AS
6:45-6:52 - ugi added to chloroform and vortexed 4 more times. Solution appears cloudy. AS
6:50 - 2mL of Acetone measured into vile and ugi product added and vortexed. CT
6:51 - Ugi product added to Acetone and vortexed. Solution appears cloudy. CT
6:52 - 2mL of Hexane measured into vile and ugi product added and vortexed. CT
6:53 - 2mL of DI water measured into vile and ugi product added and vortexed. Solution does not appear to mix. AS
6:53 - Ugi product added to Hexane. Solution appears cloudy.
6:56 - All eight solutions left in closed viles overnight to vacuum centrifuge in the morning. 2008-08-19
Objective
Ascertain the solubility of the Ugi adduct in methanol, ethanol, acetonitrile, and tetrahydrofuran.Procedure
Pipette ≈ 2mL of each solvent into four separate vials.Gradually add Ugi adduct, using sterilized (alcohol rinsed) spatula, to each vial until solution no longer remains clear once shaken.
Once excess Ugi adduct sample settles towards the bottom of the vial, filter 1mL of clear saturated liquid for speed vac assay.
Material
Solvents:
THF - Tetrahydrofuran, stabilized anhydrous 99.9%
Lot# B0307053 AcroOrganics
Methanol
Ethanol - 200 Proof
Catalog# 111 AG S200 111 USP 200 111000200 Pharmco-AAper
Acetonitrile - HPLC - 99.9%
Lot# 75-05-8 AcroOrganics
Hexane
Lot# 061507A BDH
Choloform ≈ 99%
Batch# 00751LD Sigma Aldrich
Acetone
Water (distilled)
Solute:
Ugi Product first obtained in Exp099
Results
Discussion
Cloudy solutions indicate points surpassing level of saturation.Conclusion
Log
2008-08-18
11:39 - Ugi product recrystalized ad rid of any impurities.
11:54 - Materials gathered (Methanol, Ethanol, THF, Acetonitrile)
12:30 - 2mL of methanol measured into vile and ugi product added and mixed. AS
12:32 - 2mL of acetonitrile measured into vile and ugi product added and mixed. CT
12:37 - 2mL of THF measured into vile and ugi product added and mixed. Methanol cleared up. AS
12:39 - 2mL of ethanol measured into vile and ugi product added and mixed. CT
12:41 - More ugi added to methanol. As
12:43 - More ugi added to THF. AS
12:52 - More ugi added to THF. AS. All solutions appear saturated and cloudy.
6:00 - Solutions appear saturated with residue at the bottom of the viles. Each vile vortexed to insure complete mixing.
6:40 - Gather more materials to create more saturated solutions (Deionized water, Hexane, Chloroform, Acetone)
6:44 - 2mL of Chloroform measured into vile and ugi product added and vortexed. AS
6:45-6:52 - ugi added to chloroform and vortexed 4 more times. Solution appears cloudy. AS
6:50 - 2mL of Acetone measured into vile and ugi product added and vortexed. CT
6:51 - Ugi product added to Acetone and vortexed. Solution appears cloudy. CT
6:52 - 2mL of Hexane measured into vile and ugi product added and vortexed. CT
6:53 - 2mL of DI water measured into vile and ugi product added and vortexed. Solution does not appear to mix. AS
6:53 - Ugi product added to Hexane. Solution appears cloudy.
6:56 - All eight solutions left in closed viles overnight to vacuum centrifuge in the morning.
2008-08-19
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